共查询到17条相似文献,搜索用时 12 毫秒
1.
Multilayer models of different materials were prepared and scanned. Experimental measurements are compared with mathematically predicted values. This comparison leads to a further development of multilayer models. The advantage of using a white background on a scanning table for remission measurements was confirmed by calculation and experiment. 相似文献
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Quantitative evaluation of TLC by direct photometric scanning is a promising method, in view of the development of cheap microprocessors: soon instruments for digital scanning will be commercialy available. In this paper we describe a multilayer model which seems to be a good approximation for solving the radiation transfer equation in the case of layer models with a gradient in an inward direction. Changes of remitted and transmitted light, in cases where a band lies in different layers, are presented. Examples shown are: the absorbance profile of a chromatographed band in the direction of scanning is approximated to that of an isosceles triangle; the concentration of the band is uniform, e.g. 0.3 A. U.; the concentration of the band is changing from 0 to 2.0 A. U. These results will serve to set up the correct algorithms for digital scanning and simultaneous determination in TLC. 相似文献
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Systematic and statistical errors in quantitative evaluation in TLC and HPTLC. 4. Linear calibration
Analytical results are often obtained from reflectance or fluorescence measurements in TLC or HPTLC with the aid of calibration lines. Curve fitting may not be done by conventional least squares methods for both the independent and the dependent variables are erroneous; errors occur in the volumes spotted on to the plate and in the reflectance/fluorescence measurements. Therefore the sum of the squares of the distances to the calibration line has to be minimized instead of the squared sum of the errors of the dependent variable. The algorithms used are derived and explained. Implications of error propagation for the analytical result are also given. 相似文献
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Paweł Płocharz Anna Klimek-TurekTadeusz H. Dzido 《Journal of chromatography. A》2010,1217(29):4868-4872
Kinetic performance, measured by plate height, of High-Performance Thin-Layer Chromatography (HPTLC), High-Performance Liquid Chromatography (HPLC) and Pressurized Planar Electrochromatography (PPEC) was compared for the systems with adsorbent of the HPTLC RP18W plate from Merck as the stationary phase and the mobile phase composed of acetonitrile and buffer solution. The HPLC column was packed with the adsorbent, which was scrapped from the chromatographic plate mentioned. An additional HPLC column was also packed with adsorbent of 5 μm particle diameter, C18 type silica based (LiChrosorb RP-18 from Merck). The dependence of plate height of both HPLC and PPEC separating systems on flow velocity of the mobile phase and on migration distance of the mobile phase in TLC system was presented applying test solute (prednisolone succinate). The highest performance, amongst systems investigated, was obtained for the PPEC system. The separation efficiency of the systems investigated in the paper was additionally confirmed by the separation of test component mixture composed of six hormones. 相似文献
6.
R. E. Kaiser 《Journal of separation science》1978,1(3):164-168
The principal analytical details for the third of three possible modes in high performance thin-layer chromatography are given, namely the anticircular mode. Separation is achieved by allowing the mobile phase to enter the plate layer on a precise outer circle line, from where it flows towards the centre with nearly constant speed. This technique is theoretically and practically the fastest of all three possible in HPTLC. It permits maximum sample capacity with a minimum of time, layer and mobile phase consumption. It is therefore the most economical HPTLC technique. A new carrier-free mobile phase transfer principle is used. The conditions for qualitative and quantitative analysis are good: repeatability, reproducibility and accuracy of routine TLC analyses are superior to those achieved by the classical trough technique. The specially narrow spot-path in anticircular HPTLC facilitates automated quantitation. Compared with the linear and circular modes, the anticircular mode shows better separation and significantly increased sensitivity at higher Rf-values. The drawback, however, is that the separation power (expressed by the separation number) is lower compared with the other two modes. 相似文献
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It is demonstrated that horizontai sandwich tank with two cover plates can be used to preconcentrate sample solutions. Narrow sharply-defined starting zones are obtained just outside the smaller cover plate when the series of spots of the sample solution are applied on the thin layer and predeveloped with a volatile solvent. After evaporation of the solvent, the whole area of the TLC-plate is covered with two plates and developed with a suitable solvent. 相似文献
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Circular high-performance thin-layer chromatography (HPTLC) has been used to differentiate a series of twelve tricyclic neuroleptics, using both normal phase and reverse phase procedures. The use of normal phase systems also allows the resolution of geometric isomers of chlorprothixene, clopenthixol and flupenthixol. Thirteen sulphonamides and Trirnethoprim may also be distinguished using HPTLC. 相似文献
10.
Characteristic changes in the surface topography due to UV laser treatment are of high significance for the determination of material destruction thresholds and surface structure development. E.g. irradiation of poly(ethylene terephthalate) (PET) film with pulsed UV laser light of 248 nm modifies the smoth surface of the polymer into a well oriented structured surface. The development of these structures were studied with scanning tunneling microscopy (STM) and high resolution optical profilometry. Three dimensional data of the surface were taken from the samples after each laser pulse. A change of topographic data was found in relation to fluence and number of pulses applied. © 1993 John Wilcy & Sons, Inc. 相似文献
11.
The paper discusses errors and error propagation in respect of graphic methods in quantitative in situ measurements in TLC. An error of 0.3% is possible by measuring only peak height if optimal conditions are chosen. This is in good agreement with analysis done practically which gives errors in the order of 0.3–0.6%. If the peak area is evaluated using the approximation peak height × half width, the error is in the order of 0.6%, but in real experiments only 1.5% had been found. Systematic errors in determining peak heights are introduced by the time constant of the amplifiers and the recorder. 相似文献
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P. Haefelfinger 《Journal of separation science》1979,2(1):39-42
A sensitive thin-layer chromatographic method is described for the determination of the 7–amino-metabolites of flunitrazepam and clonazepam. The same procedure is applicable to other 7-nitro-benzodiazepines such as nitrazepam. A purified plasma extract of the 7-amino-metabolites is separated by thin-layer chromatography. The primary aromatic amines are diazotized and coupled with N-(1-naphthyl) ethylene-diamine on the thin-layer plate. The quantities of the 7-amino-metabolites are directly evaluated by colorimetric densitometry. The lower limit of detection is in order of 0.5–10 ng cm?3 of plasma. The relative standard deviation of the whole procedure is less than ±15% in the range of 0.5–10 ng cm?3 for a single determination. The unchanged drugs can be reduced on the thin-layer plate and detected by the same method. Since this procedure is rather difficult to perform, it is advantageous to determine the 7-nitro-benzodiazepines in plasma by gas chromatography. The thin-layer chromatographic method was used to measure the 7-amino-metabolites in plasma of patients on either a flunitrazepam or a clonazepam oral dosing regimen. 相似文献
13.
Summary The use of 1,2-naphthoylenebenzimidazole-6-sulphochloride has been proposed as the reagent for derivatization of aliphatic amines prior to their separation, identification and quantitation both in HPLC and in TLC. The reaction of amines with this compound is quantitative and highly fluorescent derivatives are formed that provide favourable detection limits and sensitivity as compared to Dansyl derivatives of aliphatic amines. Actual detection limits achieved correspond to ca. 10–10 mol of the amine in a spot after elution from the thin-layer plate and to ca. 5·10–14 mol of the amine in a sample volume of 10 l injected into the liquid chromatograph. The use of this derivatization reagent offers good potential for the analysis of trace amounts of amines in environmental samples and in biological material.Presented at the 14th International Symposium on Chromatography London, September, 1982 相似文献
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Margit Bidl-Igly 《Journal of separation science》1978,1(3):161-163
Correlation between chemical structure and Rf-values was studied in the case of aniline and its derivatives using high performance TLC and a U-chamber. The characteristic group constants referring to each substituent were determined by chromatographing derivatives with one substituent and aniline in toluene and dibutyl ether respectively. On the basis of these constants the RM and Rf values of derivatives with more substituents were calculated. Comparing the calculated and measured values good agreement was found. 相似文献
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Rashid A. Zeineh George Kyriakidis Roger Acey Christopher Smith 《Applied biochemistry and biotechnology》1986,13(2):119-125
Citrus tristeza virus (CTV) extracted from Etrog citron (C.medica L.) was immunoprecipitated. The immunoprecipitate was fractionated by SDS-PAGE and western blotted onto nitrocellulose. The CTV
antigens were determined by immunoblot analysis using rabbit anti-CTV IgG, and the protein-band pattern exhibited on the nitrocellulose
was assessed by soft-laser scanning densitometry. The densitometric tracing revealed the presence of bands that were not visible
to the naked eye. Using the superimposition mode of the instrument, it was also revealed that the protein-band patterns of
different CTV samples were not identical. Computer-aided soft-laser scanning densitometry proved to be a powerful approach
in the detection and assessment of protein bands revealed on nitrocellulose immunoblots, which we were previously unable to
do employing conventional methods. 相似文献
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Anil K. Mukherji 《Journal of separation science》1978,1(5):273-275
Systematic studies on operation variables affecting GPC separations using the semirigid Microstyragel (Waters Associates) and the rigid silica packings (DuPont) of about equivalent porosity are reported. The dependence of (a) flow rate, (b) injection volume, and (c) concentration on elution volume and theoretical plates are examined. 相似文献